安徽农业科学2012,Vol.40Issue(10):6160-6161,6207,3.
高效液相色谱-荧光检测法测定尿中1-羟基芘
Determination of 1-Hydroxypyrene in Urine by High Performance Liquid Chromatography with Fluorescence Detection
摘要
Abstract
[ Objective ] The aim was to improve the measuring method of 1 -hydroxypyrene in urine by high performance liquid chromatography with fluorescence detection by comparing concentrated and non-concentrated eluate of C18 solid phase extraction. [ Method] Take two same urine samples, hydrolyzed by enzyme first, then enriched by C18 solid phase extraction, elution by methanol, one nitrogen dry to 1.5 ml, another direct volume to 1.5 ml, then were determined with HPLC/FLD. With Vacetnnitnle: Vwater =75 = 25 as mobile phase and 1 ml/min of flow rate, the excitation(λexI) and emission wavelengths( λem ) were 275 and 430 nm, respectively. [ Result ] The determined values of urinary 1-hydroxypyrene which after concentrating were 72.9% - 80. 6% of which non-concentrating. When use the method of non-condensed enzymatic hydrolysis high performance liquid chromatography with fluorescence detection, the limit of detection was 0.02 ng/ml, the calibration curve was linear at a given concentration range, the correlation coefficient of linear regression equation was y = 2. 404 la; - 0. 083 ( r = 0.999 9) , the recoveries were from 94.8% to 108.7% , and the average RSD was 2.7%. [ Conclusion] The method of non-condensed enzymatic hydrolysis high performance liquid chromatography with fluorescence detection can be used to determine the urine of 1-hydroyxpyrene, and it is simple, have high sensitivity and precision, good recoveries and reproducibility.关键词
浓缩/尿样/1-羟基芘/高效液相色谱Key words
Concentrate/ Human urine/ 1 -hydroxypyrene/ High performance liquid chromatography分类
农业科技引用本文复制引用
刘紫恩,何炎,张艳平,李定龙..高效液相色谱-荧光检测法测定尿中1-羟基芘[J].安徽农业科学,2012,40(10):6160-6161,6207,3.基金项目
国家环保公益性行业科研专项(200909101). (200909101)